Abstract
A novel and simple synthetic way using NaBH4 in the mixure of H2O-THF was applied to prepare 1,2-bis(diphenylphosphinoborane)ethane, dppe(BH3)2, in high yield and purity. The phosphanylborohydride compound dppe(BH3)2 was isolated in the form of colorless crystals and characterized by single crystal X-ray diffraction, 1H, 13C, 31P and 11B NMR spectroscopy. Prismatic colorless crystals of dppe(BH3)2 were obtained in monoclinic crystal system and space group P21 with two asymmetric units in the unit cell. Lattice parameters were: a = 11.657(2), b = 17.237(2), c = 12.764(2) Å, β = 98.735(14)°, 2535.0(7) Å3
Highlights
IntroductionA recent study [1] has reported the catalytic activity of ruthenium (III) acetylacetonate in the presence of different phosphorus compounds such as 1,2-bis(diphenylphosphino)ethane, dppe, in the hydrolysis of sodium borohydride
The phosphanylborohydride compound dppe(BH3)2 was isolated in the form of colorless crystals and characterized by single crystal X-ray diffraction, 1H, 13C, 31P and 11B NMR spectroscopy
Prismatic colorless crystals of dppe(BH3)2 were obtained in monoclinic crystal system and space group P21 with two asymmetric units in the unit cell
Summary
A recent study [1] has reported the catalytic activity of ruthenium (III) acetylacetonate in the presence of different phosphorus compounds such as 1,2-bis(diphenylphosphino)ethane, dppe, in the hydrolysis of sodium borohydride. At the end of catalytic reaction, in addition to the unreacted dppe, unexpectedly we isolated a new species which contains two BH3 molecules coordinated to dppe. In this catalytic reaction, NaBH4 acts as a substrate to generate hydrogen, and as a BH3 supplier in forming phosphanylborohydrides such as 1,2-bis(diphenylphosphinoborane)ethane, dppe(BH3). We report a new and simple synthetic way using NaBH4 in an homogeneous aqueous-organic solution to yield
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